Thermal analysis of water and magnesium hydroxide content in commercial pharmaceutical suspensions milk of magnesia

Journal of Thermal Analysis and Calorimetry(2012)

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摘要
A standard protocol was developed to determine the water content by thermal analysis of milk of magnesia (MoM). Differential scanning calorimetry (DSC) and thermogravimetry (TG) were used in a novel manner for examining the physical characteristics of the commercial pharmaceutical suspensions. Moisture analyzer and oven-dry methods validate the proposed protocol. MoM consists primarily of water and magnesium hydroxide [Mg(OH) 2 ]. Experimental design of the thermal analysis parameters were considered including sample size, flowing atmosphere, sample pan, and heating rate for both DSC and TG. The results established the optimum conditions for minimizing heat and mass transfer effect. Sample sizes used were: (5–15 mg) for DSC and (30–50 mg) for TG. DSC analysis used crimped crucibles with a pinhole, which allowed maximum resolution and gave well-defined mass (water) loss. TG analysis used a heating rate of 10 °C/min −1 in an atmosphere of nitrogen. The heat of crystallization, heat of fusion, and heat of vaporization of unbound water are 334, 334, and 2,257 Jg −1 , respectively (Mitra et al. Proc NATAS Annu Conf Therm Anal Appl 30:203–208, 2002 ). The DSC average water content of (MoM) was 80 wt% for name brand and 89.5 wt% for generic brand, based on the relative crystallization, melting and vaporization heats/Jg −1 of distilled water in the recently purchased (2011) MoM samples. The TG showed a two-step process, losing water at 80–135 °C for unbound water and bound water (MgO·H 2 O) at 376–404 °C, yielding a total average water loss of 91.9 % for name brand and 90.7 % for generic brand by mass. The difference between the high-temperature TG and the lower-temperature DSC can be attributed for the decomposition of magnesium hydroxide or MgO·H 2 O. Therefore in performing this new approach to water analysis by heating to a high temperature decomposed the magnesium hydroxide residue. It was determined that the TG method was the most accurate for determining bound and unbound water.
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关键词
Milk of magnesia (MoM), Differential scanning calorimetry (DSC), Thermogravimetry (TG), Unbound water and bound water
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